新显色剂对偶氮苯重氮氨基偶氮硝基苯与镉显色反应研究

报道了显色剂对偶氮苯重氮氨基偶氮硝基苯(ADAANB)在表面活性剂Tween 80和四硼酸钠介质中与镉的灵敏显色反应。在pH9.8溶液中,ADAANB最大吸收为455nm,其与镉生成的紫红色配合物最大吸收波长为566nm,表观摩尔吸光系数为1.5×105L·mol-1·cm-1。镉含量在0～16μg/25ml范围内符合比耳定律。方法可用于废水中痕量镉的测定。     

新试剂7-(苯并噻唑-2-偶氮)-8-羟基喹啉-5-磺酸的合成及与钴显色反应的研究

报道了新试剂7-(苯并噻唑-2-偶氮)-8-羟基喹啉-5-磺酸(BTHQSA)的合成方法,研究了该试剂与钴显色反应情况.结果表明,在pH3.94乙酸-乙酸钠、乳化剂OP存在下,Co-BTHQSA-OP配合物最大吸收波长为582nm,表观摩尔吸光系数ε_(582)=-5.7×10~4,钴的含量在0～12μg/25ml内,服从比耳定律.     

4,4‘—二硝基重氮氨基苯的新法合成及其与镉的显色反应研究

4,4′—二硝基重氮氨基本(DNAAB)是一种测定镉、汞等金属离子的优良的三氮烯试剂[1],其合成一般是用H2SO4—NaNO2作重氮化试剂,分重氮化和偶联两步加入反应物合成[2]。但在H2SO4作用下,NaNO2易放出NO2有毒气体。我们摸索出以亚硝酸正丁酯为重氮化试剂,以本方法合成,克服了上面缺点,并且产品纯度高,收率也较文献方法好[3]。研究了其与Cd2 的显色反应,以双峰双波长法测定,摩尔吸光系数达2.52×105L·mol-1·cm-1,用拟定方法测定了人发中镉含量,结果令人满意。1　实验部分1.1　仪器与试剂仪器:752型紫外光栅分光光度计(上海申化仪表自…     

SYNTHESIS OF A NOVEL CHELATING RESIN WITH HETEROCYCLIC RING OF S AND N

By the reaction of poly(bromoacetyl styrene) (EBPS) with thiaurea (TU), a kind of novel chelating resin with heterocyaclic ring of sulfur and nitrogen, poly[4-(2-amino)thiazoleyl-4-vinylben=ene], was synthesized. Its structure was characterized by FTIR and elemental analysis. The factors which have influence on the reaction such as reaction time, solvents, and molar ratio of reactants were investigated.     

SYNTHESIS OF A NOVEL CHELATING RESIN WITH HETEROCYCLIC RING OF S AND N

1.INTRODUCTIONThechelatingresinswithheterocyclicringofsulfur,oxygen,andnitrogenhaveexcellentadsorptionformetallicionsespeciallyfornoblemetallicions[1~3].Generally,theabove-mentionedresinsweresynthesizedbythereactionsofchloromethylatedpolystyrenewithheterocycliccompoundsinthepresenceofbase[3].Inthispaper,anewmethodforpreparingchelatingresincontaining2-amino-3-thiazoline(ATZ)wasreported.Thedetailedreactionscan2.EXPERIMENTAL2.1MaterialsEPSandBEPSweresynthesizedaccordingtothemethodde…     

SYNTHESIS OF 1-(ACETYLSALICYLYL)-BENZOTRIAZOLE AND ITS REACTION WITH POLYVINYL ALCOHOL

l-(Acetylsalicylyl)-benzotriazole, a new active amide of acetylsalicylic acid has been synthesized either from acetylsalicylic acid and benzotriazole using DCCI as condensation agent or via acetylsalicylyl chloride and benzotriazole in the presence of triethylamine. The obtained active amide reacted readily with the hydroxyl group of PVA to produce the acetylsalicylyl ester of PVA.     

1-(乙酰水杨酰)苯并三氮唑的合成及其与聚乙烯醇的反应

<正> 聚乙烯醇(PVA)作为生物相容性的水凝胶被应用在生物医用材料上。乙酰水杨酸(阿斯匹林)是一般的退烧止痛药物,近年来发现它有抗血小板凝聚的效应,但将其高分子化以制备高分子药物的工作并不多。我们曾合成了在酯基上含有阿斯匹林的五种新的丙烯酸酯单体,并进行了它们的自由基聚合,这些聚合物的水解行为表明,它们可以作为通过水解而控制释放阿斯匹林的生物相容性材料。     

新试剂1-偶氮苯基-3-(5-硝基-2-吡啶)-三氮烯的合成及其与镉的显色反应

三氮烯试剂是测定ⅠＢ、ⅡＢ族金属元素的优良试剂。近年来 ,对该类试剂中的取代苯重氮氨基苯的合成和分析应用报道较多[1 ,2 ] ,但对含杂环的三氮烯试剂的研究报道较少。我们曾将安替比林[3] 、苯并噻唑[4,5] 、噻唑[6] 引入该类试剂中 ,使试剂灵敏度有所提高。为进一步探讨此类试剂的分析性能 ,我们将 5 硝基吡啶引入 ,合成了 1 偶氮苯基 3 ( 5 硝基 2 吡啶 ) 三氮烯 (ＡＢＮＰＤＴ)。分子中含有杂环吡啶的同时还有强吸电子———ＮＯ2存在 ,另一端为具有长共轭链的偶氮苯基 ,这样更有利于试剂分子中电子的流动 ,从而改善分析性能。…     

SYNTHESIS AND CHARACTERISATION OF A NEW NIOBATE COMPLEX WITH CHROMIUM(III)

Abstract

A new hexaniobate complex with chromium(III) was prepared and characterised by analytical and spectroscopic techniques. The compound is a violet, non-crystalline solid, formulated as [Cr₂(μ-OH)(H₃Nb₆O₁₉)(en)₃(H₂O)]. It was synthesised in aqueous solution by reaction of [Cr(en)₃]³⁺, en = ethylenediammine, with the hexaniobate anion [Nb₆O₁₉]^8-, at pH 8. Thermal decomposition yielded a mixture of CrNbO₄ and Nb₂O₅. The synthesis of this compound shows that the hexaniobate anion may form complexes at lower pH values than previously reported.     

meso-四(4-磺酸基-1-萘基)卟林的合成及其与Cd(Ⅱ)显色反应研究

合成了meso-四(4-磺酸基-1-萘基)卟啉.用元素分析和红外光谱证明了产物的结构,以光度法测定了试剂在水溶液中的离解常数.在pH=7.0的六次甲基四胺的缓冲溶液中.痕量镉与试剂形成1:2的黄绿色配合物,λ_(max)=440nm,表观摩尔吸光系数ε=4.51×10~5L·mol~(-1)·cm~(-1).Cd(Ⅱ)的浓度在0～0.14μg·ml~(-1)内符合比耳定律.     

2,4-二羟基苯甲醛缩4-氨基安替比林的合成及与铝的荧光反应

合成了新荧光试剂 2 ,4 二羟基苯甲醛缩 4 氨基安替比林 (2 ,4 DHBAAP) ,并测定其结构。基于铝 (Ⅲ )与 2 ,4 DHBAAP CTMAB形成配合物 ,导致体系荧光增敏的特性 ,提出了一种测定微量铝的新荧光方法。在pH 4 .5～ 6 .0的乙酸铵缓冲溶液及CTMAB存在下 ,铝 (Ⅲ )与DHBAAP形成 1∶1的配合物。在λex λem =385 5 15nm处 ,体系产生的荧光增敏程度最大 ,铝量的线性范围为 0～ 15 0 μg·L-1,检出限为 0 .2 μg·L-1。方法用于水样中铝的测定 ,结果满意     

ADDITION REACTION OF SULFUR DICHLORIDE TO FUNCTIONALIZED IMINES DIRECTED TOWARD HETEROCYCLIC SYNTHESIS

Abstract

Although it was shown that the reactions of sulfur dichloride (SCl₂) with the imines la-c or with the azine 14 gave rise to very unstable 1 : 1 adducts, 1-aza- and 2-azabutadienes, 5 and 10, reacted with SCl₂ to afford the isothiazoles 6 and the thiazoles 11, respectively, in high yields. Addition of SCl₂ to heterocumulenes was also studied and the ketenimines 16 and diphenylketene 27 gave 1 : 1 adducts which were applied to heterocyclic synthesis as bifunctional reagents. Addition of SCl₂ to these compounds was investigated by monitoring the reactions by ¹³C nmr spectroscopy.     

显色剂4-氯-2-磺酸基苯基重氮氨基偶氮苯的合成及其与Cd(II)显色反应的研究及应用

研究了显色剂4-氯-2-磺酸基苯基重氮氨基偶氮苯(CSDAA)的理化性质及其与Cd(Ⅱ)的高灵敏度显色反应。在TritonX-100存在下,于pH10.6的氨水-氯化铵缓冲介质中,该试剂与Cd(Ⅱ)形成31的红色络合物,最大吸收波长位于521nm处,Cd(Ⅱ)在0～20μg/25ml内符合比耳定律,表观摩尔吸光系教为2.0×10     

AN UNUSUAL ADDITION AND RING-CLOSURE REACTION OF 1-(2-BROMOETHYL)-2,3-DIHYDRO- 3-PROPYL-1,3,2-BENZO-DIAZAPHOSPHORIN-4(1H)-ONE 2-OXIDE WITH CARBON DISULFIDE FOR A NEW AND CONVENIENT SYNTHESIS OF THE FUSED PHOSPHORUS HETEROCYCLIC COMPOUND

ABSTRACT

The reaction of 1-(2-bromoethyl)-2,3-dihydro-3-propyl-1,3,2-benzodiazaphosphorin-4(1H)-one 2-oxide with carbon disulfide takes an alternative pathway in the use of different bases. The sodium hydride mediated reaction leads to the formation of the tricyclic fused 1,2,3,4,4a,4b,5,6-octahydro-6-oxo-5-propyl-4-thia-3,4b,4a-thiazphosphaphenanthridine 4a-oxide via addition of H-P bond across the double bond of carbon disulfide followed by intramolecular cyclization. In the presence of triethylamine, refluxing a mixture of 1-(2-bromoethyl)-2,3-dihydro-3-propyl-1,3,2-benzodiazaphosphorin-4(1H)-one 2-oxide with carbon disulfide in benzene takes an unusual course with formation in excellent yield of the first example of fused phosphorus heterocyclic 4-[1′-(β-bromoethyl)-4′-oxo- 3′-propyl-1′,2′,3′,4′-tetrahydro-1,3,2-benzodiazaphosphorin-2′- sulfide]-1,2,3,4,4a,4b,5,6-octahydro-6-oxo-5-propyl-3,4b, 4a-thiazphosphaphenanthridine 4a,2′-dioxide, which was confirmed by spectroscopic methods, microanalyses and single crystal X-ray structure determination.     

HETEROCYCLIC PHOSPHONIUM SALTS BY REACTION OF DIMETHYL(1,2-ALKADIENYL)-PHOSPHINE OXIDES WITH ELECTROPHILIC REAGENTS

Abstract

Salts of 2,5-dihydro-1,2-oxaphosphole have been prepared by reaction of dimethyl(1,2-alkadienyl)phosphine oxides with halogens, sulfenyl and selenenyl chlorides. The essential influence of tertiary carbenium ions for realization of oxaphospholic cyclization of phosphorylated allenes has been established.     

新显色剂邻磺酸基苯偶氮若丹宁合成及与钯的光度法研究

报道了新显色剂邻磺酸基苯偶氮若丹宁（o-SBAR）的合成及其与钯显色反应的性能。在2.4mol· L~(-1)磷酸介质中,试剂与钯形成 1: 1的桔红色配合物,在 520nm波长处配合物有最大吸收,表观摩尔吸光系数为6.65×10~4,反应速度快,选择性高,应用于钯碳催化剂中钯的测定,结果满意。     

新试剂1-(4-安替比林)-3-(4-溴苯基)-三氮烯的合成及其与镉的显色反应研究

新试剂１－（４－安替比林）－３－（４－溴苯基）－三氮烯的合成及其与镉的显色反应研究佘志刚（广东药学院药学系广州５１０２２４）龚楚儒（湖北师范学院化学系黄石４３５００２关键词镉，１－（４－安替比林）－３－（４－溴苯基）－三氮烯，合成，显色反应中图分类号...     

SYNTHESIS AND STRUCTURE OF A NEW TYPE OF COORDINATION COMPOUND OF Tb（Ⅲ）WITH BENZOIC ACID

<正> The synthesis and crystal structure of a novel rare earth coordination compound are reported. [TbL3(HL)H2O]2 (HL=henzoic acid) Mr=1324. 81, triclinic, space group P1, a=9. 148(1), b=11. 4 60(2), c=13. 506(2) A ;a=112. 76(1), B=91.83(1),y=91. 99(1) ;Z=1 ;V=1303. 3(4)A3;Dc=1.69g.cm-3;F(000)= 656;u=28. 4cm-1(MoKa). The final R is 0. 024. Each rare-earth ion in the title complex is nine-coordinated by seven oxygen atoms from five benzoate groups, one benzoic acid, and one aqua molecule, forming a distorted monocapped square antiprism.     

2-(2-喹啉偶氮)-1,5-二氨基苯固相萃取光度法测定钴

合成了新试剂2 (2 喹啉偶氮) 1,5 二氨基苯(QADAB),研究了其与钴的显色反应及C18固相萃取小柱对显色络合物的固相萃取,在pH3.5磷酸盐缓冲介质中,CTMAB存在下,QADAB与钴反应生成2∶1稳定络合物,该络合物可用C18固相萃取小柱富集,小柱上富集的络合物用乙醇(内含2%乙酸)洗脱后用光度法测定,λmax=590nm,ε=8.36×104L·mol-1·cm-1。钴含量在0.01～0.80mg·L-1内符合比耳定律,方法用于环境样品中钴含量的测定,结果满意。     

新显色剂5-磺酸基[杯(4)芳烃偶氮]氨基喹啉的合成及与钯显色反应的研究

合成了新试剂 5 磺酸基 [杯 (4)芳烃偶氮 ]氨基喹啉 (SCAQ) ,研究了该试剂与钯 (Ⅱ )显色反应的适宜条件 ,在pH 8.0的缓冲介质中 ,在非离子表面活性剂TritonX 10 0存在下 ,试剂与钯(Ⅱ )生成 1∶1稳定配合物 ,建立了测定钯 (Ⅱ )的光度法新体系 ,体系至少可稳定 6h ,λmax=6 6 0nm ,ε =7.88× 10 4 L·mol- 1·cm- 1,钯 (Ⅱ )浓度在 0～ 30 μg/ 2 5ml范围内服从比耳定律。方法已用于钯催化剂中钯 (Ⅱ )的测定 ,结果与原子吸收光谱法相符 ,RSD为 1.5 %～ 2 .6 %。